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Process for the Preparation of Magnesium Nitrate Hexahydrate

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Process for the Preparation of Magnesium Nitrate Hexahydrate Patentamt JEuropaischesEuropean Patent Office ® Publication number: 0 075 354 Office européen des brevets B1 ® EUROPEAN PATENT SPECIFICATION (§) Dateof publication of patent spécification: 02.10.85 (g) Int. Cl.4: C 01 F 5/38, C 01 C 1/18 (§) Application number: 82201113.6 ® Date offiling: 09.09.82 (M) Process for the préparation of magnésium nitrate hexahydrate. (§) Priority: 17.09.81 NL 8104284 @ Proprietor: UNIE VAN KUNSTMESTFABRIEKEN B.V. Maliebaan 81 (43) Date of publication of application: NL-3581 CGUtrecht(NL) 30.03.83 Bulletin 83/13 ® Inventor: Willems, Michael Hendrik (45) Publication of the grant of the patent: Nassaustraat 9 02.10.85 Bulletin 85/40 NL-6166 BD Geleen (NL) Inventor: Vermijs, Winfried J.W. Dunantstraat 4 (84) Designated Contracting States: NL-6164GN Geleen (NL) ATBE DE FRGBIT NL SE (74) Représentative: Roeffen, Wilhelmus Johannes (§) Références cited: Msris ©t s\ GB-A-2 045 735 OCTROOIBUREAU DSM Postbus 9 US-A-1 844 862 NL-6160 MA Geleen (NL) US-A-3173 756 m m co m o o Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall Û. be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been m paid. (Art. 99(1) European patent convention). Courier Press, Leamington Spa, England. Mg(OH)2, obtained by precipitation of magnesiun compounds from sea water with dolomite The invention relates to a process for the Besides 93-96 wt.% magnesium oxide, such preparation of magnesium nitrate hexahydrate by technical-grade magnesium oxide product converting magnesium oxide with nitric acid in contains a considerable amount of impurities, the presence of water. The invention also relates particularly iron and aluminium oxides, and to a process for the preparation of thermally possibly silicon dioxide. To obtain a good stable ammonium nitrate containing granules suspension and subsequently a rapid chemical using the magnesium nitrate hexahydrate thus conversion, there is advantage in adding the obtained. magnesium oxide in finely divided form to the A process for the preparation of magnesium magnesium nitrate hexahydrate. By preference nitrate hexahydrate starting from magnesium use is made of magnesium oxide product having oxide, nitric acid and water is known from US an average particle size of at most 200 pm, in patent specification 1,844,862. According to this particular at most 100 µm, and a specific surface known process, finely divided magnesium oxide area larger than 12 m2fg. is added to dilute nitric acid whilst stirring, the For obtaining a homogeneous suspension amount added being sufficient for complete con- there further is advantage in having the suspen- version, on which the mixture is allowed to settle, sion process take place while stirring con- the solid matter is filtered off, the remaining tinuously and intensively. solution is evaporated and finally magnesium The amount of magnesium oxide suspended in nitrate hexahydrate is crystallized out by cooling. the magnesium nitrate hexahydrate may be A disadvantage of this known process is that a chosen within wide limits. For economic opera- large proportion of the impurities introduced with tion of the process, however, it is important to the magnesium oxide goes into solution, and make the amount of magnesium oxide subsequently, on cooling, to a large extent suspended in the magnesium nitrate hexahydrate crystallizes out, together with the magnesium as large as possible. Of course, this amount must nitrate hexahydrate formed, so that an impure be smaller than the maximum amount of product is obtained, which, in addition, is not magnesium oxide that is allowable in view of the easily filtered. viscosity of the suspension. In general, such an Another disadvantage of this process is that in amount is added that the magnesium oxide its practical realization always an excess of water concentration of the suspension obtained is 5-25 is introduced, which must subsequently be wt.%. removed through evaporation. According to the invention, subsequently a If this product is used in the preparation of nitric acid solution is added to the resulting thermally stable ammonium nitrate granules, it mixture, which is meanwhile being stirred. The furthermore causes severe fouling of the concentration of the nitric acid solution is chosen evaporators of the ammonium nitrate plant and, if so that practically all water introduced with the prilling is applied, it gives rise to clogging of the nitric acid and formed during the reaction is spray openings of the prilling bucket. bound as crystallization water in the resulting The present invention provides a process in magnesium nitrate hexahydrate. which the abovementioned disadvantages do not Given the gross reaction equation: or hardly occur. According to the invention this is achieved by: a) Suspending magnesium oxide in melted magnesium nitrate hexahydrate having a theoretically this would require an amount of temperature in excess of 90°C; water corresponding to the amount of water in b) Adding to the suspension obtained, whilst nitric acid with a concentration of 58.33 wt.% stirring, a nitric acid solution, resulting in the HN03. For practical purposes use is made of a formation of more magnesium nitrate nitric acid having a slightly lower concentration, hexahydrate; for instance 53-58 wt.%, in particular about 55 c) Filtering the liquid reaction mixture while wt.% HN03, because during the addition of the maintaining the temperature of the reaction acid part of the water introduced evaporates due mixture in steps (b) and (c) in excess of 90°C; to the strongly exothermic reaction that takes d) Discharging as product a part, corresponding place. to the amount of magnesium oxide introduced, of The temperature during the addition of the acid the liquid magnesium nitrate hexahydrate can be chosen within wide limits. At least this obtained as clear filtrate; temperature must be, as in the suspension e) Utilizing the remaining part as liquid medium process, 90°C, for at lower temperatures for the conversion of magnesium oxide with nitric crystallization of the magnesium nitrate hexa- acid. hydrate takes place. In the process according to the invention use Since at a high temperature the magnesium can be made of both a chemically pure and the nitrate hexahydrate decomposes into lower commercially available technical-grade hydrates or basic salts may be formed, the magnesium oxide, for instance obtained bi temperature is by preference kept below 120°C. in calcination of natural magnesite (MgC03) or c view of the large amount of reaction heat that evolves, this will generally necessitate cooling of nitrate-containing solution or melt, following the mixture during the addition of the acid. which the mixture obtained is granulated in a way The way in which the acid is added is of great known per se, optionally after evaporation. The importance in the subject process. It has been amount of magnesium nitrate hexahydrate to be found that, on the one hand, if the pH becomes added for this stabilization may vary. In general, too low (locally) because of a too large acid an amount of 0.1-1 %, in particular about 0.5 addition, various impurities, notably iron and wt.%, calculated as magnesium oxide relative to aluminium oxides, dissolve, so that they cannot the amount by weight of ammonium nitrate is be removed by filtration at a later stage, while on added. It has been found that the water content of the other hand, of course, part of the magnesium the final product obtained must be ,0.5 wt.%. oxide is not converted if the amount of acid added This can be achieved in a known way, for instance is insufficient. by evaporation of the liquid mixture to be Since it has been found that the filtration of the granulated or by drying of the granular product. mixture if favourably affected by a small amount It is true that the thermal stabilization of of non-converted magnesium oxide, by ammonium nitrate using magnesium nitrate preference use is made of such an amount of (hydrates) is known per se, see for instance the nitric acid that 92 to 98 wt.%, in particular about British patent specifications 914,606 and 988,095, 95 wt.% of the magnesium oxide introduced is but in these known processes use is made of converted into magnesium nitrate hexahydrate. water-free magnesium nitrate or lower hydrates, To eliminate the problems attaching to a too often in solution, or use is made of a magnesium large acid addition to the largest possible extent, nitrate hydrate prepared in another way than in by preference first such an amount of nitric acid is the subject process. added to the suspension that the pH of the The invention will be elucidated in the following resulting mixture is 6-6.5, this amount being examples. added at such a rate and while stirring so intensively that the reactants are homogeneously Example 1 mixed, so that the pH in the mixture locally To 600 g melted Mg(NO3)2 · 6H2O having a nowhere decreases to below about 4, and temperature of 95°C, an amount of 100 g subsequently, whilst stirring, slowly so much magnesium oxide was added, on which the nitric acid is added until a pH of 5.2-5.8 has been mixture was stirred for 15 minutes. reached in the mixture. This last addition is As magnesium oxide, use was made of a stopped when the pH decrease in the mixture, technical-grade product having an average which initially proceeds proportionally with the particle size of <75 pm and a specific surface area amount of nitric acid added, stops or proceeds of about 50 m2/g which contained 2000 ppm(*) very slowly.
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